CN101845564B - Secondary smelting method for producing magnesium-zirconium intermediate alloy - Google Patents
Secondary smelting method for producing magnesium-zirconium intermediate alloy Download PDFInfo
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Abstract
The invention discloses a secondary smelting method for producing a magnesium-zirconium intermediate alloy, which comprises the following steps of: adding 100 to 200 kg of potassium chloride into a pot, raising the temperature to between 880 and 910 DEG C in 25 to 35 minutes, and performing slagging-off; adding 60 to 195 kg of potassium fluozirconate with stirring by using a mechanical nickel rod, wherein the adding time is 10 to 30 minutes; when the furnace temperature reaches the temperature of between 880 and 910 DEG C, performing slagging-off again, and adding magnesium, wherein the addition of the magnesium is based on the weight ratio of K2ZrF6 to Mg of 1.2-1.5:1; after the magnesium is completely dissolved, spreading a protective flux, and stirring for 10 to 20 minutes by using themechanical nickel rod, standing for 4 to 10 hours, cooling to normal temperature, and brewing by using vapor and cold water; and removing and washing the slag on the alloy, performing remelting refining and slagging-off at the temperature of between 680 and 700 DEG C, and finally ingoting and testing to obtain the finished product. The secondary smelting method for producing the magnesium-zirconium intermediate alloy has the advantages of simple operation, no environmental pollution, low content of impurities in the product, a few flux impurities, high effective content of zirconium and magnesium, fine components, high uniformity, and stable performance.
Description
Technical field
The present invention relates to the production method of magnesium zirconium master alloy.
Background technology
The magnesium zirconium alloy has very favorable mechanical performance and physicals, is widely used in departments such as aircraft industry.Magnesium is the main raw material of producing the magnesium zirconium alloy.The chemically reactive of magnesium is strong, under molten state more so.It can have oxidizing reaction with oxygen, hydrogen, chlorine, sulphur and any form very soon, and with rapid oxidizing fire, therefore, melt does not need to be protected with protection flux in whole fusion-casting process, contacts with oxygen, hydrogen and furnace gas to avoid melt when bath surface does not add protection.Even also have a large amount of non-metallic inclusions to sneak into like this, Mgo, a spot of carbon, chlorine and sulfide etc. are for example arranged.Though these inclusiones are very little with the alloy phase ratio content, bring very big difficulty for the refining of alloy.Therefore, must carry out purifying treatment in process of production, how protect with flux during processing, need enough time of repose, middle operation also need be dragged for slag.
The Scientific and Technical Information Institute, Hunan Province mentions following message in novelty assessment report:
" Hunan non-ferrous metal " magazine was delivered " high zirconium magnesium zirconium master alloy technical study " literary composition 2003 the 19th the 4th phases of volume, mention a kind of method that adopts the potassium chlorate fluozirconate reduction method to produce magnesium zirconium master alloy in the literary composition, the stable content of zirconium reaches more than 30% in the alloy though this method can make, but the foreign matter content of alloy is still higher, and its quality product as shown in Figure 1.
The patent No. is 200410022059.4 patent of invention proposition " a kind of production method of magnesium zirconium master alloy ", this method need vacuumize reduction furnace and add rare gas element, zirconium tetrachloride need be vaporized, complex process, operational difficulty, difficult quality control, alloy impurity is higher, uneven components, problem of environmental pollution are difficult to solve.
Summary of the invention
The purpose of this invention is to provide a kind of secondary smelting method of producing magnesium zirconium master alloy, accomplish simple to operately, stably improve the content of zirconium, reduce the foreign matter content of alloy, make the alloying constituent homogenizing, reduce environmental pollution.
Production stage of the present invention is as follows:
1, baker: newly building or rest smelting furnace more than ten days before use must baker more than two days;
2, wash pot: will wash pot with Repone K or protection flux when the smelting furnace after block or the overhaul newly, or alloy commentaries on classics group is produced, the weight proportion of protection flux is:
Carnallitite: Calcium Fluoride (Fluorspan): SULPHUR POWDER=100: 5: 6
Charging capacity is half of steel pot capacity; When dropping into the material fusing and being warmed up to 880～910 ℃, stir secondary, emit after leaving standstill half an hour;
3, thick refining: in the steel pot, add 100～200kg Repone K, be warmed up to 880～910 ℃ in 25～30 minutes.Treat to skim after Repone K all melts, stir with mechanical nickel rod on one side the back of skimming, Yi Bian add potassium chlorate fluozirconate 60～195kg, joining day is 10～30 minutes, when being raised to 880～910 ℃ once more etc. furnace temperature, carries out skimming the second time, after this add magnesium, the add-on of magnesium is K by weight ratio
2ZrF
6: Mg=1.2～calculate at 1.5: 1;
When magnesium under 880～910 ℃ of furnace temperature all after the fusing, sprinkle protection flux, the amount of being sprinkled into is exceeded can make liquation fire extinguishing in time, stirs 10～20 minutes with mechanical nickel rod simultaneously, at this moment the steel pot is hung out;
4, dash and to boil: the fire extinguishing of one deck protection flux is spread on solution top in pot, it is left standstill be cooled to normal temperature in 4～10 hours and form crude magnesium zirconium alloy frit, dashes with steam and cold water then and boils, and dashing and boiling temperature is 80～100 ℃, with the slag inclusion on the alloy remove wash most;
5, refining remelting: will be towards the crude magnesium zirconium alloy after boiling, or add the alloy that melts down of its weight 10%, according to first chip, the caked order in back is packed in the pot, requirement adorns fine and closely, smooth, spread the SULPHUR POWDER fire extinguishing while heat then, under 680～700 ℃ of temperature condition, all be fused into alloy solution, skim this moment for the third time, and upper and lower layer all will be taken off Ex-all;
6, ingot casting: the alloy liquation was poured in the mold in 10～30 minutes, and the limit casts the limit puts out a fire with SULPHUR POWDER, and ingot is done surface dressing work after casting well;
7, check vanning: sampling 40～50 grams are chemically examined, and for (quality standard as shown in Figure 2) that composition does not reach quality standard, as melting down alloy treatment, chemically examine qualified vanning, and every case is adorned 35～45kg, dissolves with paraffin 5～6kg to cover on the finished product.
Compared with the prior art, characteristics of the present invention are to need not to vacuumize, and need not to use inertia unit body, and are simple to operate, free from environmental pollution, foreign matter content is low in the product, and flux is mingled with few, zirconium, magnesium effective content height, the composition refinement, good evenness, stable performance meets the high quality requirement of departments such as aircraft industry.
Description of drawings
Fig. 1 is the magnesium zirconium master alloy analytical quality table that existing potassium chlorate fluozirconate reduction method is produced.
Fig. 2 is the magnesium zirconium master alloy quality standard table of producing with the present invention.
Embodiment
Embodiment one
The 1st, 2,4,5,6,7 procedures are same as above in this routine production stage, and just slightly to refine operation as follows in the 3rd road: add 150kg Repone K in the steel pot, be warming up to 880～910 ℃ in 25～30 minutes.Treat to skim after Repone K all melts, add potassium chlorate fluozirconate 130kg while the back of skimming uses mechanical nickel rod to stir, the joining day is 10～30 minutes, when being raised to 880～910 ℃ once more etc. furnace temperature, carries out skimming the second time, after this adds magnesium 100kg.When magnesium under 880～910 ℃ of furnace temperature all after the fusing, sprinkle protection flux, the amount of being sprinkled into is exceeded can make liquation fire extinguishing in time, stirs 10～20 minutes with mechanical nickel rod simultaneously, at this moment the steel pot is hung out.
Embodiment two
This example and embodiment one are basic identical, and the add-on of different is magnesium is 108.3kg.
Embodiment three
This example and embodiment one are basic identical, and the add-on of different is magnesium is 86.7kg.
Embodiment four
This example is basic identical with embodiment one, and difference is that the Repone K add-on is 100kg, and the potassium chlorate fluozirconate add-on is 60kg, and the magnesium add-on is 50kg.
Embodiment five
This example is basic identical with embodiment four, and different is that the magnesium dosage is 46.2kg.
Embodiment six,
This example is basic identical with embodiment four, and different is that the magnesium add-on is 40kg.
Embodiment seven
This example is basic identical with embodiment one, and difference is that the Repone K add-on is 200kg, and the potassium chlorate fluozirconate add-on is 195kg, magnesium add-on 130kg.
Embodiment eight
This example is basic identical with embodiment seven, and different is that the magnesium add-on is 150kg.
Embodiment nine
This example is basic identical with embodiment eight, and different is that the magnesium add-on is 162.5kg..
Claims (1)
1. secondary smelting method of producing magnesium zirconium master alloy is characterized in that production stage is as follows:
A, baker: newly building or rest smelting furnace more than ten days before use must baker more than two days;
B, wash pot: newly build or overhaul after smelting furnace, or alloy commentaries on classics group will wash pot with Repone K or protection flux when producing, the weight proportion of protection flux is:
Carnallitite: Calcium Fluoride (Fluorspan): SULPHUR POWDER=100: 5: 6
Charging capacity is half of steel pot capacity, stirs secondary when dropping into the material fusing and being warmed up to 880～910 ℃, emits after leaving standstill half an hour;
C, thick refining: in the steel pot, add 100～200kg Repone K, in 25～35 minutes, be warming up to 880～910 ℃, treat to skim after Repone K all melts, skim the back on one side with the stirring of mechanical nickel rod, Yi Bian add potassium chlorate fluozirconate 60～195kg, the joining day is 10～30 minutes, when being raised to 880～910 ℃ once more etc. furnace temperature, carry out skimming the second time, after this add magnesium, the add-on of magnesium is K by weight ratio
2ZrF
6: Mg=1.2～calculate at 1.5: 1; When magnesium is all sprinkling protection flux after the fusing under 880～910 ℃ of furnace temperature, the amount of being sprinkled into is exceeded can make liquation fire extinguishing in time, stirs 10～20 minutes with mechanical nickel rod simultaneously, at this moment the steel pot is hung out;
D, dash and to boil: the fire extinguishing of one deck protection flux is spread on solution top in pot, it is left standstill be cooled to normal temperature in 4～10 hours and form crude magnesium zirconium alloy frit, dashes with steam and cold water then and boils, and dashing and boiling temperature is 80～100 ℃, with the slag inclusion on the alloy remove wash most;
E, refining remelting: will be towards the crude magnesium zirconium alloy after boiling, or add the alloy that melts down of its weight 10%, pack in the pot according to first chip, the caked order in back, requirement adorns fine and closely, smooth, spread the SULPHUR POWDER fire extinguishing then while heating, all be fused into alloy solution under 680～700 ℃ of temperature condition, skim this moment for the third time, and upper and lower layer all will be taken off Ex-all;
F, ingot casting: the alloy liquation was poured in the mold in 10～30 minutes, and the limit casts the limit puts out a fire with SULPHUR POWDER, and ingot is done surface dressing work after casting well;
G, check vanning: sampling 40～50 grams are chemically examined, and do not reach quality standard for composition, as melting down alloy treatment; Chemically examine qualified vanning, every case is adorned 35～45Kg, dissolves with paraffin 5～6kg to cover on the finished product.
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| CN1580302A (en) * | 2004-05-21 | 2005-02-16 | 锦州市金属材料研究所 | Method for producing magnesium-zirconium inter mediate alloy |
| CN1639389A (en) * | 2002-01-18 | 2005-07-13 | 铸造中心有限公司 | Magnesium-zirconium alloying |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1639389A (en) * | 2002-01-18 | 2005-07-13 | 铸造中心有限公司 | Magnesium-zirconium alloying |
| CN1580302A (en) * | 2004-05-21 | 2005-02-16 | 锦州市金属材料研究所 | Method for producing magnesium-zirconium inter mediate alloy |
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